CN110412183A - A kind of needle trapping-gas chromatography-mass spectrography is to rose aroma analysis of components method - Google Patents
A kind of needle trapping-gas chromatography-mass spectrography is to rose aroma analysis of components method Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of rose aroma analysis of components methods of needle trapping-gas chromatography-mass spectrography.Needle trapping is a kind of Sample Pretreatment Technique of advanced solvent free, after the rose of fresh and field cultivation is placed in ml headspace bottle, heating device is opened to be heated, trapping needle insertion ml headspace bottle is adsorbed, then trapping needle is extracted from ml headspace bottle, it is inserted into gas chromatography-mass spectrum injection port to be desorbed, passes through gas chromatography-mass spectrum qualitative analysis after desorption.The present invention uses continuous adsorption process, is greatly improved the bioaccumulation efficiency of sample, volatile component in sample is overflowed from sample, traps adsorption sampling using trapping needle, detector is entered after desorption and is analyzed, the sampling analysis suitable for trace organic target component.Can enriched with trace component, high sensitivity, adsorption range be wide, favorable reproducibility, easy to operate.Salable preservation after absorption, by-product is few in adsorption process, and qualitative, quantitative is accurate, easy to operate, lasts a long time.
Description
Technical field
The present invention relates to a kind of needle trapping-gas chromatography-mass spectrographies to rose aroma analysis of components method.
Background technique
Rose (Rosa rugosa Thunb) is rosaceae rose, and it is main to have become hotan area at present
The industrial crops of plantation become one of Xinjiang characteristic product.Rose gives off a strong fragrance pure, refreshing, is extracted by its petal
Essential oil is referred to as " liquid golden ", can be widely applied to the industries such as food, chemical industry, medical treatment.Rose is with economic value and sight
The plant for appreciating value, can be medicinal and edible, is used as medicine with bud, is one of China's rare medicinal herbs, has toxin-expelling and face nourishing, promoting the circulation of qi living
Blood, stagnation resolvation of having one's ideas straightened out, it is soothing the liver be amusing, promote bile secretion, is aid digestion, adjust body the effect of.Bud, the fresh flower of rose are fragrant with it
Gas is fragrant and sweet, strong plentiful and self-contained style, rose variety are numerous, cold-resistant, drought-enduring, adaptable.Studies have shown that different sources
Rose oil pump capacity and fragrance component have a great difference.Kind is the essential oil of rose variety an important factor for influencing derived essential oil
Using must be set up in fully understanding to derived essential oil.But during preparing essential oil using rose, it is related to
The escape or recombination of a part of ingredient such as further investigate fresh flower head space volatile ingredient, more will appreciate that rose variety volatilizees
The natural constituents of object.Currently, common head space method has solid phase microextraction and electronic nose.6:108-111 modern science in 2013
The scholars such as instrument Qian Zongyao utilize the volatile component in headspace solid-phase microextraction technology absorption hotan rose, chromatography-
Mass spectrometric hyphenated technique analyzes and identifies its chemical component, is normalized with peak area quantitative.Test is isolated from rose
18 peaks identify 16 kinds of chemical components therein, account for the 95.88% of total peak area.2016 34 (4): 57-64 Shanghai traffic
College journal (agricultural sciences version) Song Wanyao etc. extracts 2 kinds of domestic roses using 2 kinds of methods of organic solvent extraction and solid phase microextraction
Volatile component in rare water.Gas chromatography mass spectrometer analysis shows, in 2 kinds of rose waters that Solid-phase Microextraction is obtained by extraction
Fragrance component type (respectively 31 kinds and 28 kinds) is significantly more than the fragrance component type (difference that organic solvent extractionprocess extracts
For 23 kinds and 21 kinds).Scholars utilize electronic nose and gas-chromatography-matter around in 2:1-6 fragrance flavor and cosmetic in 2017 etc.
Spectrometer is to the fresh rose flower of 3 " living body " Chinese bitter water rose, Bulgarian powder rose and Arabescato Normal rose different cultivars
Fragrance is studied.3 kinds of roses identify 26 kinds of volatile components altogether.Chinese bitter water rose identifies 22 kinds of volatile components,
Arabescato Normal rose identifies 23 kinds of volatile components, and the pink rose of Bulgaria identifies 14 kinds of volatile components.2018
46 (9): 204-207 Jiangsu's agriculture science Yuan Ying etc. utilizes headspace solid-phase microextraction and gas phase using rich colored rose as research object
Chromatograph-mass spectrometer coupling technology measures rich colored rose and opens phase, full-bloom stage in bud stage, just, is volatilized under 4 kinds of flowering phases of fallen flowers phase
The relative amount variation of the type and each volatile ingredient divided.Bud stage detects 43 kinds of volatile ingredients altogether, just opens the phase and detects 54 altogether
Kind volatile ingredient, full-bloom stage detect 59 kinds of volatile ingredients altogether, detect 56 kinds of volatile ingredient altogether in the fallen flowers phase.2018 08,
20 (4): pure wait of 22-25 Anshan Normal University journal Li Tie extracts dry, fresh-rose wave using headspace solid-phase microextraction technology
Hair property ingredient, through Gas Chromatography-Mass Spectrometry, comparative analysis is dry, fresh-rose aroma component changes.Wherein in dried rose
18 kinds of volatile compounds are identified, 18 kinds of volatile compounds are identified from fresh-rose.2018 37 (2): 26-
The scholars such as text are had detected edible using solid phase microextraction and Gas chromatographyMass spectrometry in 32 Chinese Wild plant resources
Fragrance ingredient of the rose variety ' Yunnan black tea ' in 3 period flowers such as bud stage, half-open phase and phases in full bloom.85 kinds of chemistry are identified altogether
Ingredient has 38 kinds, 47 kinds, 40 kinds in the classes of compounds that bud stage, 3 periods of half-open phase and phase in full bloom separate identification respectively.
And to the enrichment of rose head space other than solid phase microextraction and electronic nose, the development of needle trapping also provides a kind of letter for its research
Just, fast, accurately method.It is had not been reported currently, needle is captured in the application in rose and Rosa Damascana.
Needle method of trapping is that active adsorbing and trapping samples and solid phase microextraction is before the sample of one for one kind novel being integrated with
Processing technique.Its working principle is that being coated with the hollow trapping needle of specific single-layer or multi-layer adsorbent in inner wall using one, make needle
It is connected with syringe or sampling pump, passes through gas sample in needle by outer power when sampling, target analytes are adsorbed concentration, then
Trapping needle is inserted into gas-chromatography high temperature injection port, the analysis component being sucked out through pyrolysis is brought into chromatographic column, realizes sample
The separation of object is analyzed.Currently, trapping needle is mainly used in the enrichment of volatile organic matter.2010 29 (5): 508-512
The scholars such as rock and mineral testing magazine height pine just trap 7 kinds of benzene homologues in adsorbing and extracting underground water with needle, with headspace sampling gas-chromatography
Method measurement, method recovery of standard addition, detection limit and precision meet Environmental Protection Agency relevant criterion.Analytical chemistry in 2012
Research report 40 (9): 1353-1359 high pine etc. has studied closed cycle Dynamic headspace-needle trapping analysis underground based on ultrasound
The method of nitrobenzene and aniline in water, the results showed that the trapping of one layer of adsorbent of filling is lower than for the residual of object
0.79%, the detection of aniline is limited to 2.9-3.7g/L, and the detection of nitrobenzene is limited to 0.7-1.9g/L.The recycling of aniline and nitrobenzene
Rate reaches preferable analytical effect between 83%-113%.2018 analysis tests journal 37 (6): 708-713 Li Yuan root etc. is built
The method for having found volatile chemical component in closed cycle dynamic needle trapping/Gas Chromatography-Mass Spectrometry cigarette shreds, from identification
Compound amounts and total peak area out, relative standard deviation and to comparing in terms of the enrichment of low boiling point volatile component
Compared with the sensitivity of Trapping ways, repeatability are superior to solid phase microextraction.Needle trapping is applied to natural plants side by some scholars
Face, Yunnan University's journal (natural science edition) 37 (2) in 2015: the identical application dynamic needle trapping-gas chromatography mass spectrometry method of 265-271 Wu
Volatile component from 3 Shilin Park, Yunnan, China, Dehong and Xishuangbanna planting site peppermints is analyzed, the peppermint produced from stone forest
Middle separation identifies 28 kinds of chemical components, and mass fractions relative accounts for the 97.19% of the gross area；Also divide from the peppermint that Dehong produces
From 28 kinds of chemical components are identified, mass fractions relative accounts for the 90.11% of the gross area；It is separated from the peppermint that is produced from Xishuangbanna
26 kinds of chemical components are identified, mass fractions relative accounts for the 93.92% of the gross area.Research has shown that needle trapping has enrichment temperature
With efficiently, parsing easily and fast, the advantages that high sensitivity, long service life.Chinese experimental pharmacology of traditional Chinese medical formulae magazine 24 in 2018
(21): 120-128 Qin Yan et al. identifies volatile component 112 using needle method of trapping altogether from viola mandshurica, predominantly in
Etc. volatile ingredient, and Static Headspace method therefrom identifies volatile component 37, predominantly high volatile ingredient altogether.
Rose fragrance component is equal by many factors such as kind, the place of production, weather, collecting time, cultivation condition and storage times
Have an impact, forefathers have used extraction by steam distillation Rosa Damascana and using headspace solid-phase microextraction to its volatile component
It is characterized.To fully understand that its volatile component, the fragrance component of more simple, fast and efficient research rose more have
Necessity using a variety of methods be especially novel sample-pretreating method to rose carry out in-depth study, for and field rose into
The development of one step provides technical support.
Summary of the invention
The object of the present invention is to provide a kind of needle trapping-gas chromatography-mass spectrographies to rose aroma analysis of components
Method after the rose that fresh and field is cultivated is placed in ml headspace bottle by this method, is opened heating device and is heated, in temperature 60
DEG C heating 30min after, will trapping needle insertion ml headspace bottle adsorb, then will trapping needle extracted from ml headspace bottle, be inserted into gas
Phase chromatography-mass spectroscopy injection port is desorbed, and passes through gas chromatography-mass spectrum qualitative analysis after desorption.The present invention is inhaled using continuous
Attached process is greatly improved the bioaccumulation efficiency of sample, and volatile component in sample is overflowed from sample, is trapped using trapping needle
Adsorption sampling enters detector and analyzes after desorption, the sampling analysis suitable for trace organic target component.It can enriched with trace group
Point, high sensitivity, adsorption range be wide, favorable reproducibility, easy to operate.Salable preservation after absorption, by-product is few in adsorption process, fixed
Property it is quantitative accurate, it is easy to operate, last a long time.Overcome the shortcomings of that existing rose measurement pre-treatment is time-consuming, Extracting temperature is high.
A kind of needle trapping-gas chromatography-mass spectrography of the present invention presses rose aroma analysis of components method
Column step carries out:
The analysis of dynamic needle trapping:
A, it takes fresh and field cultivation rose to smash to pieces, weighs 1g sample in screw thread mouth ml headspace bottle of the 20mL with dottle pin, add
Enter 500 microlitres of saturated sodium chloride solutions, is put into heating balance 30min in the head space heater of 30-80 DEG C of constant temperature of temperature, will be coated with
2,6 dibenzofuran porous polymeric resins, three kinds of adsorbent 60-80 mesh of ketjenblack EC adsorbent and carbon molecular sieve；Poly- diformazan
Radical siloxane adsorbent 100-120 mesh, divinyl benzene adsorbent 80-120 mesh and three kinds of carbon molecular sieve adsorbent 60-80 mesh suctions
Attached dose；Or 2,6 dibenzofuran porous polymeric resins 60-80 mesh, dimethyl silicone polymer adsorbent 100-120 mesh and carbon molecules
In the trapping needle insertion bottle of three kinds of adsorbents of sieve adsorbant 60-80 mesh, 1mm below pin hole to dottle pin connects trapping needle other end
It is connected on Portable sampling device, and opens battery voltage switch, volume flow is then set as 8-12mL/min, volume is set as
18-22mL finally presses start button, is enriched with 1-3min, after being enriched with 20mL volume, removes trapping needle and is put into gas chromatographic sample introduction
Mouthful, constant temperature parses 4min under the conditions of 250 DEG C of temperature；
The analysis of gas-chromatography:
B, using Agilent 7890B-5977A type gas chromatography mass spectrometer, chromatographic column is in HP-5MS 30m × 0.25mm
Diameter, 0.25 μm of film thickness, chromatographic condition are as follows: 240-260 DEG C of temperature of gas chromatographic sample introduction mouth, sample introduction mode using not shunt mode into
Row, column oven temperature program: after holding 0.3-0.7 minutes of 30-40 DEG C of initial temperature, is warming up to 170-190 DEG C with 2-4 DEG C/min
It is kept for 0 minute, then is warming up to 190-210 DEG C with 4-6 DEG C/min and is kept for 0 minute, then 240-260 is warming up to 18-22 DEG C/min
It DEG C is kept for 2-4 minute, using constant current mode, carrier gas is the helium of purity > 99.9995%, flow velocity 0.9- for sample operation
1.1mL/min；
Mass spectrographic analysis:
C, electron impact ion source, electron collision energy are 70eV, and ion source temperature is 220-240 DEG C, transmission line temperature
It is 140-160 DEG C, 240-260 DEG C of auxiliary temperature；Acquisition quality number range is 40-500amu；Mass analyzer: level four bars；It sweeps
Retouch mode: full scan, solvent-free delay.
A kind of needle trapping-gas chromatography-mass spectrography of the present invention is to rose aroma analysis of components method, the party
The advantages of method and good effect are as follows: needle trapping is a kind of Sample Pretreatment Technique of advanced solvent free, when due to its sampling
Gas sample is passed through in needle by outer power, target analytes are adsorbed concentration, it is thereby achieved that low temperature or normal temperature enrichment,
The chemical component in natural plants will not be destroyed, the oxidation of high temperature bring and decomposition is avoided, there is very high fidelity effect.
It is filled in dynamic needle using different materials, extraction selectivity multiplicity, along with sampling pump continuously works, enrichment effect
Fruit is better than other pretreatment technologies.The ingredient adsorbed in conjunction with gas chromatography-mass spectrum to it carries out qualitative analysis, meets Rose Essentielle
Gas ingredient is qualitative.
A kind of needle trapping-gas chromatography-mass spectrography of the present invention is to rose aroma analysis of components method, the party
Method is suitable for the qualitative analysis of rose aroma component:
Table 1,2,3 is and the main component table of rose aroma ingredient is cultivated in field, and trapping needle type is respectively that needle inner wall applies
2,6 dibenzofuran porous polymeric resins of cloth, three kinds of adsorbent (60-80 of ketjenblack EC adsorbent and carbon molecular sieve adsorbent
Mesh)；Dimethyl silicone polymer adsorbent (100-120 mesh), divinyl benzene adsorbent (80-120 mesh) and carbon molecular sieve absorption
Three kinds of adsorbents of agent (60-80 mesh)；2,6 dibenzofuran porous polymeric resins (60-80 mesh), dimethyl silicone polymer adsorbent
(100-120 mesh) and three kinds of adsorbents of carbon molecular sieve adsorbent (60-80 mesh).
Detailed description of the invention
Fig. 1 is present example sample and fresh rose aroma ingredient total ion current figure, trapping needle type point are cultivated in field
Not Wei needle inner wall be coated with 2,6 dibenzofuran porous polymeric resins, ketjenblack EC adsorbent and three kinds of carbon molecular sieve adsorbent
Adsorbent (60-80 mesh).
Fig. 2 is present example sample and fresh rose aroma ingredient total ion current figure, trapping needle type point are cultivated in field
It Wei not needle inner wall coating dimethyl silicone polymer adsorbent (100-120 mesh), divinyl benzene adsorbent (80-120 mesh) and carbon
Three kinds of adsorbents of adsorbent of molecular sieve (60-80 mesh).
Fig. 3 is present example sample and fresh rose aroma ingredient total ion current figure, trapping needle type point are cultivated in field
Not Wei needle inner wall be coated with 2,6 dibenzofuran porous polymeric resins (60-80 mesh), dimethyl silicone polymer adsorbent (100-120
Mesh) and three kinds of adsorbents of carbon molecular sieve adsorbent (60-80 mesh).
Specific embodiment
With reference to the accompanying drawing, invention is further described in detail for main component table and specific embodiment:
Instrument: U.S.'s Agilent 7890B-5977A gas chromatograph-mass spectrometer (GC-MS).The trapping of SC-045-XL-19 type needle
Portable sampling device, including 1-50mL/min electronic flow controller, constant temperature heating device, vacuum sampling pump, sampling controller.
The trapping needle of three kinds of different absorbent coatings: needle inner wall is coated with 2,6 dibenzofuran porous polymeric resins, graphitized carbon
Three kinds of adsorbents of black adsorbent and carbon molecular sieve adsorbent (60-80 mesh)；Needle inner wall is coated with dimethyl silicone polymer adsorbent
(100-120 mesh), three kinds of adsorbents of divinyl benzene adsorbent (80-120 mesh) and carbon molecular sieve adsorbent (60-80 mesh)；Or
Needle inner wall is coated with 2,6 dibenzofuran porous polymeric resins (60-80 mesh), dimethyl silicone polymer adsorbent (100-120 mesh)
With three kinds of adsorbents of carbon molecular sieve adsorbent (60-80 mesh)；Head space screw thread mouth sample bottle of the 20mL with dottle pin.
Reagent: sodium chloride is analyzed pure；Secondary distilled water.
Embodiment 1
The analysis of dynamic needle trapping:
A, it takes fresh and field cultivation rose to smash to pieces, weighs 1g sample in screw thread mouth ml headspace bottle of the 20mL with dottle pin, add
Enter 500 microlitres of saturated sodium chloride solutions, is placed in heating balance 30min in the head space heater of temperature 60 C constant temperature, 2,6 will be coated with
Dibenzofuran porous polymeric resins, three kinds of adsorbents of ketjenblack EC adsorbent and carbon molecular sieve adsorbent (60-80 mesh)
It traps in needle insertion bottle, trapping needle other end is connected on Portable sampling device, and opens electricity by 1mm below pin hole to dottle pin
Then volume flow is set as 10mL/min by pond group voltage switch, volume is set as 20mL, finally presses start button, is enriched with 2min,
After being enriched with 20mL volume, removes trapping needle and be put into gas chromatographic sample introduction mouth, constant temperature parses 4min under the conditions of 250 DEG C of temperature；Through
Gas chromatography-mass spectrometry analysis, Comprehensive analysis results obtain fresh rose aroma ingredient result；
The analysis of gas-chromatography:
B, using Agilent 7890B-5977A type gas chromatography mass spectrometer, chromatographic column is in HP-5MS 30m × 0.25mm
Diameter, 0.25 μm of film thickness, chromatographic condition are as follows: 240 DEG C of gas chromatographic sample introduction mouth temperature, sample introduction mode are carried out using not shunt mode,
Column oven temperature program: after 35 DEG C of initial temperature are kept for 0.5 minute, 180 DEG C is warming up to 3 DEG C/min and is kept for 0 minute, then with 5
DEG C/min be warming up to 200 DEG C keep 0 minute, then with 20 DEG C/min be warming up to 250 DEG C keep 3 minutes, sample operation use constant current
Mode, carrier gas are the helium of purity > 99.9995%, flow velocity 1.0mL/min；
Mass spectrographic analysis:
C, electron impact ion source, electron collision energy are 70eV, and ion source temperature is 230 DEG C, and transmission line temperature is 150
DEG C, 250 DEG C of auxiliary temperature；Acquisition quality number range is 40-500amu；Mass analyzer: level four bars；Scan pattern: full scan,
Solvent-free delay.
The NIST11 library searching that the total ion current figure that gas chromatograph-mass spectrometer is obtained is carried by system, and combine
Related document carries out artificial spectrum elucidation, determines the title of each ingredient of rose fragrance.By chem workstation data processing system,
The percentage contents of each chemical component are acquired by area normalization method, concrete outcome is shown in Table 1；
The main component table of table 1 and field cultivation rose aroma ingredient: trapping needle type is that needle inner wall is coated with 2,6 hexichol furans
It mutters porous polymeric resins, three kinds of adsorbents of ketjenblack EC adsorbent and carbon molecular sieve
Embodiment 2
The analysis of dynamic needle trapping:
A, it takes fresh and field cultivation rose to smash to pieces, weighs 1g sample in screw thread mouth ml headspace bottle of the 20mL with dottle pin, add
Enter 500 microlitres of saturated sodium chloride solutions, is put into heating balance 30min in the head space heater of temperature 60 C constant temperature, it is poly- by being coated with
Dimethyl siloxane adsorbent (100-120 mesh), divinyl benzene adsorbent (80-120 mesh) and carbon molecular sieve adsorbent (60-
80 mesh) three kinds of adsorbents trapping needle insertion bottle in, 1mm below pin hole to dottle pin, will trapping needle other end be connected to it is portable
On sampler, and battery voltage switch is opened, volume flow is then set as 10mL/min, volume is set as 20mL, finally presses
Start button is enriched with 2min, after being enriched with 20mL volume, removes trapping needle and is put into gas chromatographic sample introduction mouth, in 250 DEG C of conditions of temperature
Lower constant temperature parses 4min；Through gas chromatography-mass spectrometry analysis, Comprehensive analysis results obtain fresh rose aroma ingredient result；
The analysis of gas-chromatography:
B, using Agilent 7890B-5977A type gas chromatography mass spectrometer, chromatographic column is in HP-5MS 30m × 0.25mm
Diameter, 0.25 μm of film thickness, chromatographic condition are as follows: 250 DEG C of gas chromatographic sample introduction mouth temperature, sample introduction mode are carried out using not shunt mode,
Column oven temperature program: after 35 DEG C of initial temperature are kept for 0.5 minute, 180 DEG C is warming up to 3 DEG C/min and is kept for 0 minute, then with 5
DEG C/min be warming up to 200 DEG C keep 0 minute, then with 20 DEG C/min be warming up to 250 DEG C keep 3 minutes, sample operation use constant current
Mode, carrier gas are the helium of purity > 99.9995%, flow velocity 1.0mL/min；
Mass spectrographic analysis:
C, electron impact ion source, electron collision energy are 70eV, and ion source temperature is 230 DEG C, and transmission line temperature is 150
DEG C, 250 DEG C of auxiliary temperature；Acquisition quality number range is 40-500amu；Mass analyzer: level four bars；Scan pattern: full scan,
Solvent-free delay.
The NIST11 library searching that the total ion current figure that gas chromatograph-mass spectrometer is obtained is carried by system, and combine
Related document carries out artificial spectrum elucidation, determines the title of each ingredient of rose fragrance.By chem workstation data processing system,
The percentage contents of each chemical component are acquired by area normalization method, concrete outcome is shown in Table 2；
The main component table of table 2 and field cultivation rose aroma ingredient: trapping needle type is that needle inner wall is coated with poly dimethyl
Siloxanes adsorbent, divinyl benzene adsorbent and carbon molecular sieve adsorbent
Embodiment 3
The analysis of dynamic needle trapping:
A, it takes fresh and field cultivation rose to smash to pieces, weighs 1g sample in screw thread mouth ml headspace bottle of the 20mL with dottle pin, add
Enter 500 microlitres of saturated sodium chloride solutions, is put into heating balance 30min in the head space heater of temperature 60 C constant temperature, 2,6 will be coated with
Dibenzofuran porous polymeric resins (60-80 mesh), dimethyl silicone polymer adsorbent (100-120 mesh) and carbon molecular sieve absorption
In the trapping needle insertion bottle of three kinds of adsorbents of agent (60-80 mesh), trapping needle other end is connected to by 1mm below pin hole to dottle pin
On Portable sampling device, and battery voltage switch to be opened, volume flow is then set as 10mL/min, volume is set as 20mL,
Start button is finally pressed, 2min is enriched with, after being enriched with 20mL volume, trapping needle is removed and is put into gas chromatographic sample introduction mouth, in temperature 250
Constant temperature parses 4min under the conditions of DEG C；Through gas chromatography-mass spectrometry analysis, Comprehensive analysis results obtain fresh rose aroma ingredient knot
Fruit；
The analysis of gas-chromatography:
B, using Agilent 7890B-5977A type gas chromatography mass spectrometer, chromatographic column is in HP-5MS 30m × 0.25mm
Diameter, 0.25 μm of film thickness, chromatographic condition are as follows: 260 DEG C of gas chromatographic sample introduction mouth temperature, sample introduction mode are carried out using not shunt mode,
Column oven temperature program: after 35 DEG C of initial temperature are kept for 0.5 minute, 180 DEG C is warming up to 3 DEG C/min and is kept for 0 minute, then with 5
DEG C/min be warming up to 200 DEG C keep 0 minute, then with 20 DEG C/min be warming up to 250 DEG C keep 3 minutes, sample operation use constant current
Mode, carrier gas are the helium of purity > 99.9995%, flow velocity 1.0mL/min；
Mass spectrographic analysis:
C, electron impact ion source, electron collision energy are 70eV, and ion source temperature is 230 DEG C, and transmission line temperature is 150
DEG C, 250 DEG C of auxiliary temperature；Acquisition quality number range is 40-500amu；Mass analyzer: level four bars；Scan pattern: full scan,
Solvent-free delay.
The NIST11 library searching that the total ion current figure that gas chromatograph-mass spectrometer is obtained is carried by system, and combine
Related document carries out artificial spectrum elucidation, determines the title of each ingredient of rose fragrance.By chem workstation data processing system,
The percentage contents of each chemical component are acquired by area normalization method, concrete outcome is shown in Table 3；
The main component table of table 3 and field cultivation rose aroma ingredient: trapping needle type is that needle inner wall is coated with 2,6 hexichol furans
It mutters porous polymeric resins, dimethyl silicone polymer adsorbent and carbon molecular sieve adsorbent
Utilize the method for the present invention, using 2,6 dibenzofuran porous polymeric resins, ketjenblack EC adsorbent and carbon molecules
The trapping needle for sieving three kinds of adsorbents identifies 51 chromatographic peaks altogether, and qualitative chromatographic peak area out accounts for the 98.83% of the gross area；Make
With dimethyl silicone polymer adsorbent, the trapping needle of three kinds of adsorbents of divinyl benzene adsorbent and carbon molecular sieve identifies 64 altogether
A chromatographic peak, qualitative chromatographic peak area out account for the 99.17% of the gross area；Using 2,6 dibenzofuran porous polymeric resins, gather
The trapping needle of three kinds of adsorbents of dimethyl siloxane adsorbent and carbon molecular sieve identifies 50 chromatographic peaks, qualitative chromatography out altogether
Peak area accounts for the 83.38% of the gross area；Wherein, dimethyl silicone polymer adsorbent, divinyl benzene adsorbent and carbon molecular sieve
The trapping of three kinds of adsorbents has preferable concentration effect for field cultivation rose, can be used for subsequent rose and rhodamine toner
The further qualitative and quantitative analysis of oil.
Claims (1)
1. a kind of needle trapping-gas chromatography-mass spectrography is to rose aroma analysis of components method, it is characterised in that press following step
It is rapid to carry out:
The analysis of dynamic needle trapping:
A, it takes fresh and field cultivation rose to smash to pieces, weighs 1 g sample in screw thread mouth ml headspace bottle of 20 mL with dottle pin, be added
500 microlitres of saturated sodium chloride solutions are put into heating balance 30min in the head space heater of 30-80 DEG C of constant temperature of temperature, will be coated with 2,
6 dibenzofuran porous polymeric resins, three kinds of adsorbent 60-80 mesh of ketjenblack EC adsorbent and carbon molecular sieve；Poly dimethyl
Siloxanes adsorbent 100-120 mesh, divinyl benzene adsorbent 80-120 mesh and three kinds of carbon molecular sieve adsorbent 60-80 mesh absorption
Agent；Or 2,6 dibenzofuran porous polymeric resins 60-80 mesh, dimethyl silicone polymer adsorbent 100-120 mesh and carbon molecular sieve
In the trapping needle insertion bottle of three kinds of adsorbents of adsorbent 60-80 mesh, 1 mm below pin hole to dottle pin, by the connection of trapping needle other end
In on Portable sampling device, and battery voltage switch is opened, volume flow is then set as 8-12 mL/min, volume is set as
18-22 mL, finally press start button, be enriched with 1-3 min, be enriched with 20 mL volumes after, remove trapping needle be put into gas-chromatography into
Sample mouth, constant temperature parses 4 min under the conditions of 250 DEG C of temperature；
The analysis of gas-chromatography:
B, using Agilent 7890B-5977A type gas chromatography mass spectrometer, chromatographic column is HP-5MS 30 m × 0.25 mm internal diameter,
0.25 μm of film thickness, chromatographic condition are as follows: 240-260 DEG C of temperature of gas chromatographic sample introduction mouth, sample introduction mode using not shunt mode into
Row, column oven temperature program: after holding 0.3-0.7 minutes of 30-40 DEG C of initial temperature, is warming up to 170-190 with 2-4 DEG C/min
It DEG C is kept for 0 minute, then is warming up to 190-210 DEG C with 4-6 DEG C/min and is kept for 0 minute, then 240- is warming up to 18-22 DEG C/min
260 DEG C holding 2-4 minutes, sample operation use constant current mode, carrier gas is the helium of purity > 99.9995%, flow velocity 0.9-
1.1 mL/min；
Mass spectrographic analysis:
C, electron impact ion source, electron collision energy are 70 eV, and ion source temperature is 220-240 DEG C, and transmission line temperature is
140-160 DEG C, 240-260 DEG C of auxiliary temperature；Acquisition quality number range is 40-500 amu；Mass analyzer: level four bars；Scanning
Mode: full scan, solvent-free delay.
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